ASTM D4530-03
(Test Method)Standard Test Method for Determination of Carbon Residue (Micro Method)
Standard Test Method for Determination of Carbon Residue (Micro Method)
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (see Note 1) formed after evaporation and pyrolysis of petroleum materials under certain conditions and is intended to provide some indication of the relative coke forming tendency of such materials.
1.2 The test results are equivalent to the Conradson Carbon Residue test (see Test Method D 189).
Note1—This procedure is a modification of the original method and apparatus for carbon residue of petroleum materials, where it has been demonstrated that thermogravimetry is another applicable technique. However, it is the responsibility of the operator to establish operating conditions to obtain equivalent results when using thermogravimetry.
1.3 This test method is applicable to petroleum products that partially decompose on distillation at atmospheric pressure and was tested for carbon residue values of 0.10 to 30 % (m/m). Samples expected to be below 0.10 weight % (m/m) residue should be distilled to remove 90 % (V/V) of the flask charge (see Section ). The 10 % bottoms remaining is then tested for carbon residue by this test method.
1.4 Ash-forming constituents, as defined by Test Method D 482, or non-volatile additives present in the sample will add to the carbon residue value and be included as part of the total carbon residue value reported.
1.5 Also in diesel fuel, the presence of alkyl nitrates, such as amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher carbon residue value than observed in untreated fuel, which may lead to erroneous conclusions as to the coke-forming propensity of the fuel. The presence of alkyl nitrate in the fuel may be detected by Test Method D 4046.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety practices and to determine the applicability of regulatory limitations prior to use. For specific warning statements, see 8.2.3 and 8.4.
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An American National Standard
Designation:D4530–03
Standard Test Method for
1
Determination of Carbon Residue (Micro Method)
This standard is issued under the fixed designation D 4530; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* priate safety practices and to determine the applicability of
regulatory limitations prior to use. For specific warning
1.1 This test method covers the determination of the amount
statements, see 8.2.3 and 8.4.
of carbon residue (see Note 1) formed after evaporation and
pyrolysis of petroleum materials under certain conditions and
2. Referenced Documents
is intended to provide some indication of the relative coke
2.1 ASTM Standards:
forming tendency of such materials.
D 189 Test Method for Conradson Carbon Residue of
1.2 The test results are equivalent to the Conradson Carbon
3
Petroleum Products
Residue test (see Test Method D 189).
3
D 482 Test Method for Ash from Petroleum Products
NOTE 1—This procedure is a modification of the original method and
D 4046 Test Method for Alkyl Nitrate in Diesel Fuels by
apparatus for carbon residue of petroleum materials, where it has been
4
Spectrophotometry
2
demonstrated that thermogravimetry is another applicable technique.
D 4057 Practice for Manual Sampling of Petroleum and
However, it is the responsibility of the operator to establish operating
4
Petroleum Products
conditions to obtain equivalent results when using thermogravimetry.
D 4177 Practice for Automatic Sampling of Petroleum and
1.3 Thistestmethodisapplicabletopetroleumproductsthat
4
Petroleum Products
partially decompose on distillation at atmospheric pressure and
5
E 1 Specification for ASTM Thermometers
was tested for carbon residue values of 0.10 to 30 % (m/m).
6
E 133 Specification for Distillation Equipment
Samples expected to be below 0.10 weight % (m/m) residue
2.2 IP Standard:
should be distilled to remove 90 % (V/V) of the flask charge
7
Specification for IP Standard Thermometers
(see Section 9). The 10 % bottoms remaining is then tested for
carbon residue by this test method.
3. Terminology
1.4 Ash-forming constituents, as defined by Test Method
3.1 Definitions:
D 482, or non-volatile additives present in the sample will add
3.1.1 carbon residue, n—in petroleum products, the part
to the carbon residue value and be included as part of the total
remaining after a sample has been subjected to thermal
carbon residue value reported.
decomposition.
1.5 Alsoindieselfuel,thepresenceofalkylnitrates,suchas
3.1.1.1 Discussion—The amount of residue is dependent on
amyl nitrate, hexyl nitrate, or octyl nitrate, causes a higher
the test conditions of evaporation and pyrolysis. The term may
carbon residue value than observed in untreated fuel, which
be misleading here in that the residue may contain other than
may lead to erroneous conclusions as to the coke-forming
carbon decomposition products. However, the term is retained
propensity of the fuel. The presence of alkyl nitrate in the fuel
due to its wide common usage.
may be detected by Test Method D 4046.
1.6 The values stated in SI units are to be regarded as the
4. Summary of Test Method
standard. The values given in parentheses are for information
4.1 A weighed quantity of sample is placed in a glass vial
only.
and heated to 500°C under an inert (nitrogen) atmosphere in a
1.7 This standard does not purport to address all of the
controlled manner for a specific time. The sample undergoes
safety concerns, if any, associated with its use. It is the
coking reactions, and volatiles formed are swept away by the
responsibility of the user of this standard to establish appro-
3
Annual Book of ASTM Standards, Vol 05.01.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on Annual Book of ASTM Standards, Vol 05.02.
5
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 14.03.
6
D02.06 on Analysis of Lubricants. Annual Book of ASTM Standards, Vol 14.04.
7
Current edition approved May 10, 2003. Published June 2003. Originally Methods forAnalysis and Testing, Institute of Petroleum Standard Methods for
approved in 1985. Last previous edition approved in 2000 as D 4530–00. Petroleum and Its Products, Part I, Vol 2. Available from Institute of Petroleum, 61
2
See Fuel, Vol 63, July 1984, pp. 931–934. New Cavendish St., London, WIM 8AR, UK.
*A Summary of Changes section appears at the end of this standard.
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